Zirconium silicate assisted removal of residual proteins after organic solvent deproteinization of human plasma,enhancing the stability of the LC–ESI-MS response for the bioanalysis of small molecules

An efficient blood plasma clean-up method was developed, where methanol protein precipitation was applied, followed by zirconium silicate assisted exclusion of residual proteins. A strong binding of zirconium (IV) silicate to the proteins enabled the elimination of remaining proteins after solvent deproteinization through a rapid solid-phase extraction (SPE) procedure. Matrix-assisted laser desorption/ionization time-of-flight mass spectrometry (MALDI/TOF MS) was used for monitoring the proteins during clean-up practice applied to human plasma samples. The proteins were quantified by colorimetric detection using the bicinchoninic acid (BCA) assay. The presented analytical strategy resulted in the depletion of >99.6% proteins from human plasma samples. Furthermore, high-performance liquid chromatography hyphenated to diode-array and electrospray ionization mass spectrometric detection (HPLC–DAD/ESI MS) was applied for qualitative and quantitative analysis of the caffeoylquinic acids (CQAs) and their metabolites in human plasma. The procedure demonstrated high recoveries for the standard compounds spiked at different concentrations. Cynarin and chlorogenic acid were recovered in the range of 81–86% and 78–83%, respectively. Caffeic acid was extracted in the excess of 89–92%, while ferulic acid and dihydroxyhydrocinnamic acid showed a recovery of 87–91% and 92–95%, respectively. The method was partially validated in accordance with FDA-Industry Guidelines for Bioanalytical Method Validation (2001). The presented scheme improves the clean-up efficacy of the methanol deproteinization, significantly reduces the matrix effects and provides a great analytical tool for the isolation of small molecules from human plasma.     

Recent progress of poly (N-isopropylacrylamide) hybrid hydrogels: synthesis,fundamentals and applications – review

Hydrogels, having nanomaterials (e.g. nanoparticles and nanorods) incorporated inside their polymeric meshes, are generally called hybrid gels/hydrogels. These assemblies combine the properties of both hydrogels and nanomaterials in one system. These responsive hybrid hydrogels, particularly polymerized N-isopropylacrylamide (PoNip) polymeric gels, have been extensively exploited for various multi-disciplinary applications in the literature over the past two decades because of their unique and exquisite particulars. Next generation assemblies have been prepared by using the smart nature of these gels toward the general incentives (e.g. temperature, ionic strength, and pH) in the fields of nanocatalysis, water purification, drug delivery, photonics, and optics. This review presents an overview of the PoNip hybrid assemblies engineered over the past 7 years i.e. 2010–2016 and extensively discusses the interaction of the incorporated nanomaterial with the polymeric chains of the hydrogels as it is the most significant factor which makes these assemblies attractive for all the associated applications. Moreover, this article also describes the preparative routes, properties, classification, and applications of these hybrid hydrogels in the fields of medicine, environment, catalysis, and nanotechnology.     

Structures and Bioactivities of Steroidal Saponins Isolated from the Genera Dracaena and Sansevieria

The species Dracaena and Sansevieria, that are well-known for different uses in traditional medicines and as indoor ornamental plants with air purifying property, are rich sources of bioactive secondary metabolites. In fact, a wide variety of phytochemical constituents have been isolated so far from about seventeen species. This paper has reviewed the literature of about 180 steroidal saponins, isolated from Dracaena and Sansevieria species, as a basis for further studies. Saponins are among the most characteristic metabolites isolated from the two genera. They show a great variety in structural motifs and a wide range of biological activities, including anti-inflammatory, anti-microbial, anti-proliferative effects and, in most case, remarkable cytotoxic properties.     

Studies on thermal oxidation of chalcopyrite from Chitradurga,Karnataka State,India

When chalcopyrite is heated in air, up to 350? there is no marked change. Between 350 and 440?, surface material is oxidised to iron sulphate, CuSO₄ and Fe₂O₃, while in regions not accessible to oxygen the formation of Cu₅FeS₄, FeS and S takes place. From 440 to 500? oxidation and sulphation phenomena occur. Stable compounds between 500 and 650? are iron sulphate, CuSO₄ and Fe₄O₃, with a minor amount of 6CuO.Cu₂O indicated at 650?. After the decomposition of iron sulphate, CuSO₄ decomposes, first to CuO.CuSO₄ and then to CuO. By 750? the sulphur has been totally lost from all compounds, while the oxides of copper and iron partly react to form CuFe₂O₄. Final products of oxidation between 800 and 850? are CuO, CuFe₂O₄ and Fe₃O₄.     

The role of various binding materials for trace elemental analysis of powder samples using laser-induced breakdown spectroscopy

Study of various binding materials like potassium bromide, poly(vinyl alcohol), starch, silver and aluminum has been carried out using laser-induced breakdown spectroscopy (LIBS). The role of matrix effects using these five binders on LIBS signal intensity was investigated for better performance of LIBS technique as a quantitative analytical tool. For comparative study of different binders, the signal intensity of different Mg lines at 518.3, 517.2, 383.8 and 279.5 nm wavelengths were recorded for pellets prepared with known concentrations of Mg in these binders. The influence of laser energy on ablated mass under different binding materials and its correlation with LIBS signal intensity has been explored. Optical scanning microscopy images of the ablated crater were studied to understand the laser ablation process. The study revealed that the binding material plays an important role in the generation of LIBS signal. The relative signal intensity measured for a standard Mg line (at 518.3 nm) were 735, 538, 387, 227 and 130 for potassium bromide, starch, poly(vinyl alcohol), silver and aluminum as binders, respectively. This indicates clearly that potassium bromide is better as a binder for LIBS studies of powder samples.     

Synthesis,characterization and biological properties of novel ON donor bidentate Schiff bases and their copper(II) complexes

Four novel ON donor Schiff bases (E)-3-((4-phenoxyphenylimino)methyl)benzene-1,2-diol (HL₁),(E)-3-((4-(4-biphenyloxy)phenyliminomethyl)benzene-1,2-diol (HL₂), (E)-3-((4-naphthoxyphenylimino)methyl)benzene-1,2-diol (HL₃), (E)-3-((4-(2-naphthoxy)phenylimino)methyl)benzene-1,2-diol (HL₄) and their copper(II) complexes bis((E)-3-((4-phenoxyphenylimino)methyl)benzene-1,2-diol) copper(II) (Cu(L₁)₂) bis((E)-3-((4-(4-biphenyloxy)phenylimino)methyl)benzene-1,2-diol) copper(II) (Cu(L₂)₂), bis((E)-3-((4-naphthoxyphenylimino)methyl)benzene-1,2-diol) copper(II) (Cu(L₃)₂), bis((E)-3-((4-(2-naphthoxy)phenylimino)methyl)benzene-1,2-diol) copper(II) (Cu(L₄)₂) have been synthesized and characterized by spectroscopic (FTIR, NMR, UV–visible) and elemental analysis. The crystal structures of HL₁, HL₂, HL_3, and HL₄ have been determined, which reveal intramolecular N-H?O (HL₁, HL₂, HL_3, and HL₄) hydrogen bonds in the solid state. Keto-amine and enol-imine tautomerism is exhibited by the Schiff bases in solid and solution states. The Schiff bases and their copper(II) complexes have been screened for their biological activities. In antimicrobial assays (antibacterial and antifungal), HL₄ showed promising results against all strains through dual inhibition property while the rest of the compounds showed activity against selective strains. On the other hand, in cytotoxic, DPPH, and inhibition of hydroxyl (OH) free radical-induced DNA damage assays, the results were found significantly correlated with each other, i.e. the ligands HL₁ and HL₂ showed moderate activity while their complexes Cu(L₁)₂ and Cu(L₂)₂ exhibited prominent increase in activity. As the results of these assays are supporting each other, it represents the strong positive correlation and antioxidant nature of investigated compounds.     

A review on <Superscript>90</Superscript>Y-labeled compounds and biomolecules

The field of therapeutic nuclear medicine is emerging rapidly as choice of treatment in oncology and other cellular malignancies. The growth of this branch of nuclear medicine is greatly facilitated by the introduction of a number of new radiopharmaceuticals and radionuclides. ⁹⁰Y-radiopharmaceuticals have confirmed their worth in medical and clinical areas in a very short span of time. The ⁹⁰Y is a radioisotope widely used for therapeutic purposes and considerable perfection has been made to understand the chemistry of ⁹⁰Y-labeled radiopharmaceuticals. The development of these radiopharmaceuticals can be made favorable by using appropriate buffer, incubation period, optimal pH, specific activity and reaction temperature. In this review, we have discussed the preparation of range of ⁹⁰Y transporting biological molecules such as antibodies radiolabeled peptides, antigens and microsphere with their clinical applications.     

Structural,compositional and hardness properties of hydrogenated amorphous carbon nitride thin films synthesized by dense plasma focus device

The hydrogenated amorphous carbon nitride (a‐CN_x:H) thin films were synthesized on the SS‐304 substrates using a dense plasma focus device. The a‐CN_x:H thin films were synthesized using CH₄/N₂ admixture gas and 20 focus deposition shots on substrates placed at different distances from the anode top. X‐ray photoelectron spectroscopy and Raman analysis confirmed different C–N bonding in the a‐CN_x:H thin films. A decrease in the N/C ratio as well as the sp³/sp² ratio with an increase in the substrate distance has been observed. The higher amount of C–N formation for the film synthesized at 10 cm is observed which decreases with increasing distance. The X‐ray photoelectron spectroscopy and Raman analysis affirmed the C ≡ N presence in all the thin films synthesized at different distances. The morphology of the synthesized a‐CN_x:H thin films showed nanoparticles and nanoparticle clusters formation at the surface. The hardness results showed comparatively lower hardness of the a‐CN_x:H thin films due to the presence of C ≡ N. The C–N formation with lower amount of C ≡ N and a higher N/C ratio as well as a higher sp³/sp² ratio for the films synthesized at 10 cm show reasonably higher hardness. Copyright © 2016 John Wiley & Sons, Ltd.     

Fabrication of Sensitive Potentiometric Cholesterol Biosensor Based on Co3O4 Interconnected Nanowires

Highly sensitive, selective, reliable and inexpensive cholesterol biosensors are highly demanded for the routine monitoring of cholesterol molecules in order to prevent heart failure incidents. In this study, Co₃O₄ nanostructures are synthesized using polyvinyl pyrrolidone surfactant as growth template by a low temperature aqueous chemical growth method. The morphology of nanostructures was investigated by scanning electron microscopy and X‐ray diffraction techniques. The nanostructures exhibit interconnected nanowires like morphology with interconnected network of nanowires. The nanostructures of Co₃O₄ are polycrystalline. The cholesterol oxidase was physically adsorbed on the interconnected nanowires of Co₃O₄ for the chemical sensing of cholesterol molecules. The sensor device detected a wide range of cholesterol from 1×10^?7 M to 1×10^?3 M concentrations with sensitivity of ?94.031 mV/decade. A detection limit of 0.035×10^?7 M cholesterol concentration was observed and a fast response time of 10 s was also noticed. The fabricated device is highly stable, selective, sensitive, reproducible and repeatable. All the collected information about presented cholesterol biosensor indicates its potential application for the monitoring of cholesterol concentrations from human blood serum and real‐life samples.